摘要
目的 建立测定D-苯甘氨酸甲酯盐酸盐中手性异构体(L-苯甘氨酸甲酯盐酸盐)含量的高效液相色谱(HPLC)方法。方法 采用CHIRALPAK IA手性色谱柱(250 mm×4.6 mm,5μm);以正己烷-异丙醇-二乙胺(920:80:1)为流动相,检测波长为230 nm,流速0.8 ml/min,柱温30℃。结果 空白溶剂无干扰,分离度符合规定。检测限为0.6μg/ml,定量限为1.3μg/ml。L-苯甘氨酸甲酯在1.3~37.6μg/ml范围内,溶液的浓度与峰面积呈良好的线性关系(y=0.119x-0.046,r=0.998>0.99),平均回收率为104.3%(RSD<10.0%,n=9)。结论该方法操作简便,专属性强,灵敏度高,可有效检出D-苯甘氨酸甲酯盐酸盐中手性异构体的含量,适用于其手性杂质的控制。
Objective To establish an HPLC method for the quantitative analysis of chiral isomer(L-phenylglycine methyl ester) in D-phenylglycine methyl ester hydrochloride.Methods CHIRALPAK IA(250 mm×4.6 mm,5 μm)was adopted,using n-hexane-isopropyl alcohol-diethylamine(920:80:1) at a flow rate of 0.8 ml/min as mobile phase.The detection wavelength was 230 nm and the column temperature was 30 ℃.Results The blank solvent had no interference,and the resolution met the requirements.The LOD and LOQ were 0.6 μg/ml and 1.3 μg/ml,respectively.The concentration of L-phenylglycine methyl ester solution had a good linear relationship with the peak area in the concentration range of 1.3-37.6 μg/ml(y=0.119x-0.046,r=0.9980.99).The average recovery was 104.3 %,with RSD<10.0 %(n=9).Conclusion The method is simple,specific and sensitive for the determination of optical isomer in D-phenylglycine methyl ester hydrochloride,thus is suitable for the control of its chiral impurity.
作者
许鑫
刘蕊
孔令兰
王艳梅
XU Xin;LIU Rui;KONG Ling-lan;WANG Yan-mei(Shandong Lukang Pharmaceutical Co.,Ltd.,Jining 272100,China)
出处
《食品与药品》
CAS
2023年第2期192-192,I0004,I0005,共3页
Food and Drug
